CN109979639A - A kind of nano chips encapsulation mixed type conductive silver paste - Google Patents

A kind of nano chips encapsulation mixed type conductive silver paste Download PDF

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Publication number
CN109979639A
CN109979639A CN201910119183.1A CN201910119183A CN109979639A CN 109979639 A CN109979639 A CN 109979639A CN 201910119183 A CN201910119183 A CN 201910119183A CN 109979639 A CN109979639 A CN 109979639A
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China
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silver powder
nano
silver paste
type conductive
mixed type
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CN201910119183.1A
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Chinese (zh)
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崔建中
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Anglo Nanoscale Polytron Technologies Inc
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Anglo Nanoscale Polytron Technologies Inc
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Priority to CN201910119183.1A priority Critical patent/CN109979639A/en
Publication of CN109979639A publication Critical patent/CN109979639A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20Conductive material dispersed in non-conductive organic material
    • H01B1/22Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00Apparatus or processes specially adapted for manufacturing conductors or cables

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Nanotechnology (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Dispersion Chemistry (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Conductive Materials (AREA)
  • Powder Metallurgy (AREA)

Abstract

The present invention provides a kind of nano chips encapsulation mixed type conductive silver pastes, and preparation method of the present invention is simple, and preparation process condition is reliable and stable, no pollution to the environment;The present invention includes silver powder 65%-85%, organic solvent 5%-25%, dispersing agent 1%-2%, organic carrier 10%-20%, surfactant 0.5%-5%, diluent 0.1%-5%;By rosin acid as surfactant, acrylic resin and ethyl cellulose mixture as organic carrier, the generation for effectively having delayed the generation of mass diffusion and having prevented low temperature non-dense setization from spreading, the stabilization to keep particle is mixed with micro-silver powder using nano-silver powder, play dispersing nanoparticles, the effect reunited is prevented, the performance of silver paste is improved;The silver paste of receiving for using the formula of the application and preparation method to obtain simultaneously is sintered later thermal conductivity as 193W/ (Km), better than the heating conduction for the heat-conducting glue and solder for being commonly used to encapsulation at present, the shear strength of sintered joint can achieve 37.5MPa, have excellent performance.

Description

A kind of nano chips encapsulation mixed type conductive silver paste
Technical field
The present invention relates to chip encapsulation technology fields, and in particular to a kind of nano chips encapsulation mixed type conductive silver paste.
Background technique
Due to the use limitation in world wide about solder containing pb in electronic package interconnections, electronics is unleaded to be always The emphasis of electronic interconnection research, current main lead-free solder are the alloys such as Sn-Ag-Cu, Sn-Cu and Au-Sn, but compared to Pb-Sn solder, the lead-free solder disadvantage high there are still such as poor processability and processing temperature.On the other hand, high-power broadband Being widely used for gap chip and sharply increasing so that requirement of the package system to heat dissipation is higher and higher, for core for power density The mutual hot glue of chip level interconnection and the heating conduction of solder cannot increasingly be met the requirements.Nanometer is mutually linked as electronic package interconnections Provide another unleaded solution.Due to dimensional effect, the fusing point and sintering temperature of nano particle are far below block material Material.The nano particle of surface melting, which is sintered together to ultimately form by the effect of liquid phase capillary force, has melt similar to block materials The agglomerated material of point.There is metallic silver very high thermal conductivity to allow it to the heat dissipation performance for meeting high power density system, because This nano-Ag particles is in electronic package interconnections as the alternative materials of solder.But nano-Ag particles are thermodynamically normal It plays pendulum, leads to interparticle reunion, this reunion will lead to the uneven dispersion of nano-Ag particles, thus be formed Macroscopic void significantly reduces starting powder density before sintering, and effective radius is more much larger than real radius, when effective radius reaches When micron order, the advantage of nano-Ag particles just without.
Summary of the invention
In order to solve the problems in the existing technology, the present invention provides a kind of nano chips encapsulation mixed type conductions Silver paste has the characteristics that reducing nano-Ag particles reunites.
Technical proposal that the invention solves the above-mentioned problems are as follows: a kind of nano chips encapsulation mixed type conductive silver paste, by weight Measure percentages, including silver powder 65%-85%, organic solvent 5%-25%, dispersing agent 1%-2%, organic carrier 10%- 20%, surfactant 0.5%-5%, diluent 0.1%-5%;
Silver paste the preparation method is as follows:
(1) by weight percentage, it weighs silver powder 65%-85%, organic solvent 5%-25%, dispersing agent 1%-2%, have Airborne body 10%-20%, surfactant 0.5%-5%, diluent 0.1%-5%;
(2) organic solvent water-bath is heated to 50 DEG C -80 DEG C, is slowly added into dispersing agent, organic carrier, diluent, it is mechanical It stirs evenly, obtains solution A;
(3) after solution A is cooling, silver powder is poured into solution A, after mechanical stirring 20min, obtains solution B;
(4) beaker equipped with solution B is put into ultrasound 10min-30min in Ultrasound Instrument, 15 DEG C of the water temperature holding-of Ultrasound Instrument 28 DEG C and sonic oscillation it is fully dispersed, be uniformly mixed obtain silver paste.
(5) it will will be put into three-roll grinder and be ground uniformly, while part organic solvent being made to volatilize, it is viscous to increase silver paste Degree.
Further, silver powder includes micro-silver powder and nano-silver powder, and micro-silver powder average diameter is 0.5 μm -3 μm, nanometer Silver powder purity is 99.99%, and nano-silver powder average grain diameter is 20nm;The mass ratio of micro-silver powder and nano-silver powder is 1:8.
Further, organic solvent is one of methanol, ethyl alcohol, acetone.
Further, the anhydrous citric acid sodium that dispersing agent is polyvinylpyrrolidone or purity is 98%.
Further, organic carrier is the mixture of acrylic resin and ethyl cellulose, wherein acrylic resin and second The mass ratio of base cellulose is 11:4.
Further, surfactant is rosin acid.
Further, diluent is terpinol.
The present invention has the utility model has the advantages that preparation method of the present invention is simple, and preparation process condition is reliable and stable, to environment without dirt Dye;By rosin acid as surfactant, acrylic resin and ethyl cellulose mixture as organic carrier, effectively The generation for having delayed the generation of mass diffusion and having prevented low temperature non-dense setization from spreading, is mixed using nano-silver powder with micro-silver powder The stabilization of particle is kept, dispersing nanoparticles are played the role of, prevents from reuniting, improves the performance of silver paste;This Shen is used simultaneously It is 193W/ (Km) that silver paste that formula please and preparation method obtained receive, which is sintered later thermal conductivity, better than being commonly used at present The heat-conducting glue of encapsulation and the heating conduction of solder, the shear strength of sintered joint can achieve 37.5MPa, have excellent performance.
Specific embodiment
The present invention is further illustrated With reference to embodiment.
Embodiment 1
A kind of nano chips encapsulation mixed type conductive silver paste by weight percentage, including silver powder 65%-85%, has Solvent 5%-25%, dispersing agent 1%-2%, organic carrier 10%-20%, surfactant 0.5%-5%, diluent 0.1%-5%;
Silver paste the preparation method is as follows:
(1) by weight percentage, silver powder 70% is weighed, silver powder includes micro-silver powder and nano-silver powder, and micro-silver powder is flat Equal diameter is 1 μm, and nano-silver powder purity is 99.99%, and nano-silver powder average grain diameter is 20nm;Micro-silver powder and nano-silver powder Mass ratio is 1:8;Ethyl alcohol 10%;Polyvinylpyrrolidone 1.5%;Organic carrier 15%, organic carrier be acrylic resin and The mixture of ethyl cellulose, wherein the mass ratio of acrylic resin and ethyl cellulose is 11:4;Rosin acid 0.5%;Rosin Alcohol 3%;
(2) by alcohol solvent heating water bath to 60 DEG C, it is fine that polyvinylpyrrolidone, acrylic resin and ethyl are slowly added into Mixture, the abienol of element are tieed up, mechanical stirring is uniform, obtains solution A;
(3) after solution A is cooling, silver powder is poured into solution A, after mechanical stirring 20min, obtains solution B;
(4) beaker equipped with solution B is put into ultrasound 20min in Ultrasound Instrument, the water temperature of Ultrasound Instrument keeps 20 DEG C and ultrasound Vibrate it is fully dispersed, be uniformly mixed obtain silver paste.
(5) it will will be put into three-roll grinder and be ground uniformly, while part organic solvent being made to volatilize, it is viscous to increase silver paste Degree.
Embodiment 2
A kind of nano chips encapsulation mixed type conductive silver paste by weight percentage, including silver powder 65%-85%, has Solvent 5%-25%, dispersing agent 1%-2%, organic carrier 10%-20%, surfactant 0.5%-5%, diluent 0.1%-5%;
Silver paste the preparation method is as follows:
(1) by weight percentage, silver powder 80% is weighed, silver powder includes micro-silver powder and nano-silver powder, and micro-silver powder is flat Equal diameter is 1 μm, and nano-silver powder purity is 99.99%, and nano-silver powder average grain diameter is 20nm;Micro-silver powder and nano-silver powder Mass ratio is 1:8;Acetone 5%;Polyvinylpyrrolidone 1%;Organic carrier 10%, organic carrier are acrylic resin and second The mixture of base cellulose, wherein the mass ratio of acrylic resin and ethyl cellulose is 11:4;Rosin acid 1%;Abienol 3%;
(2) by alcohol solvent heating water bath to 60 DEG C, it is fine that polyvinylpyrrolidone, acrylic resin and ethyl are slowly added into Mixture, the abienol of element are tieed up, mechanical stirring is uniform, obtains solution A;
(3) after solution A is cooling, silver powder is poured into solution A, after mechanical stirring 20min, obtains solution B;
(4) beaker equipped with solution B is put into ultrasound 20min in Ultrasound Instrument, the water temperature of Ultrasound Instrument keeps 25 DEG C and ultrasound Vibrate it is fully dispersed, be uniformly mixed obtain silver paste.
(5) it will will be put into three-roll grinder and be ground uniformly, while part organic solvent being made to volatilize, it is viscous to increase silver paste Degree.
Embodiment 3
A kind of nano chips encapsulation mixed type conductive silver paste by weight percentage, including silver powder 65%-85%, has Solvent 5%-25%, dispersing agent 1%-2%, organic carrier 10%-20%, surfactant 0.5%-5%, diluent 0.1%-5%;
Silver paste the preparation method is as follows:
(1) by weight percentage, silver powder 70% is weighed, silver powder includes micro-silver powder and nano-silver powder, and micro-silver powder is flat Equal diameter is 1 μm, and nano-silver powder purity is 99.99%, and nano-silver powder average grain diameter is 20nm;Micro-silver powder and nano-silver powder Mass ratio is 1:8;Acetone 10%;Polyvinylpyrrolidone 1%;Organic carrier 15%, organic carrier are acrylic resin and second The mixture of base cellulose, wherein the mass ratio of acrylic resin and ethyl cellulose is 11:4;Rosin acid 2%;Abienol 2%;
(2) by alcohol solvent heating water bath to 70 DEG C, it is fine that polyvinylpyrrolidone, acrylic resin and ethyl are slowly added into Mixture, the abienol of element are tieed up, mechanical stirring is uniform, obtains solution A;
(3) after solution A is cooling, silver powder is poured into solution A, after mechanical stirring 20min, obtains solution B;
(4) beaker equipped with solution B is put into ultrasound 20min in Ultrasound Instrument, the water temperature of Ultrasound Instrument keeps 25 DEG C and ultrasound Vibrate it is fully dispersed, be uniformly mixed obtain silver paste.
(5) it will will be put into three-roll grinder and be ground uniformly, while part organic solvent being made to volatilize, it is viscous to increase silver paste Degree.
The sintering temperature of the application is 300 DEG C, and sintering process is heated to 280 DEG C with the heating rate of 5 DEG C/min, when heat preservation Between be 10-60min, be sintered later thermal conductivity be 193W/ (Km), better than be commonly used at present encapsulation heat-conducting glue and alloy The shear strength of the heating conduction of solder, sintered joint can achieve 37.5MPa
Many other changes and remodeling can be made by not departing from the spirit and scope of the present invention.It should be appreciated that the present invention is not It is limited to specific embodiment, the scope of the present invention is defined by the following claims.

Claims (7)

1. a kind of nano chips encapsulation mixed type conductive silver paste, which is characterized in that by weight percentage, including silver powder 65%-85%, organic solvent 5%-25%, dispersing agent 1%-2%, organic carrier 10%-20%, surfactant 0.5%- 5%, diluent 0.1%-5%;
Silver paste the preparation method is as follows:
(1) by weight percentage, weigh silver powder 65%-85%, organic solvent 5%-25%, dispersing agent 1%-2%, have it is airborne Body 10%-20%, surfactant 0.5%-5%, diluent 0.1%-5%;
(2) organic solvent water-bath is heated to 50 DEG C -80 DEG C, is slowly added into dispersing agent, organic carrier, diluent, mechanical stirring Uniformly, solution A is obtained;
(3) after solution A is cooling, silver powder is poured into solution A, after mechanical stirring 20min, obtains solution B;
(4) beaker equipped with solution B is put into ultrasound 10min-30min in Ultrasound Instrument, the water temperature of Ultrasound Instrument is kept for 15 DEG C -28 DEG C With sonic oscillation it is fully dispersed, be uniformly mixed obtain silver paste.
(5) it will will be put into three-roll grinder and be ground uniformly, while part organic solvent being made to volatilize, and increase silver paste viscosity.
2. a kind of nano chips encapsulation mixed type conductive silver paste as described in claim 1, which is characterized in that the silver powder packet Micro-silver powder and nano-silver powder are included, micro-silver powder average diameter is 0.5 μm -3 μm, and nano-silver powder purity is 99.99%, nano silver Powder average grain diameter is 20nm;The mass ratio of micro-silver powder and nano-silver powder is 1:8.
3. a kind of nano chips encapsulation mixed type conductive silver paste as described in claim 1, which is characterized in that described organic molten Agent is one of methanol, ethyl alcohol, acetone.
4. a kind of nano chips encapsulation mixed type conductive silver paste as described in claim 1, which is characterized in that the dispersing agent The anhydrous citric acid sodium for being 98% for polyvinylpyrrolidone or purity.
5. a kind of nano chips encapsulation mixed type conductive silver paste as described in claim 1, which is characterized in that it is described have it is airborne Body is the mixture of acrylic resin and ethyl cellulose, and wherein the mass ratio of acrylic resin and ethyl cellulose is 11:4.
6. a kind of nano chips encapsulation mixed type conductive silver paste as described in claim 1, which is characterized in that the surface is living Property agent be rosin acid.
7. a kind of nano chips encapsulation mixed type conductive silver paste as described in claim 1, which is characterized in that the diluent For terpinol.
CN201910119183.1A 2019-02-18 2019-02-18 A kind of nano chips encapsulation mixed type conductive silver paste Pending CN109979639A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111354514A (en) * 2020-03-06 2020-06-30 深圳第三代半导体研究院 Packaging paste based on multi-dimensional nano material and preparation method thereof
CN113284645A (en) * 2021-04-25 2021-08-20 广州汉源新材料股份有限公司 Nano silver paste and preparation method thereof
CN114334221A (en) * 2022-01-10 2022-04-12 珠海方正科技多层电路板有限公司 Hole plugging copper paste, preparation method thereof and printed circuit board
CN115810439A (en) * 2022-12-02 2023-03-17 广东华智芯电子科技有限公司 Silver-containing composite slurry, preparation method thereof and electronic interconnection material
CN116313223A (en) * 2023-03-28 2023-06-23 深圳市众诚达应用材料科技有限公司 Silver colloid and preparation method thereof

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CN102290117A (en) * 2011-04-25 2011-12-21 深圳市唯特偶新材料股份有限公司 Low temperature-sintered nano silver paste and preparation method thereof
CN102646459A (en) * 2012-05-23 2012-08-22 湖南利德电子浆料有限公司 Silver paste for front face of mixed silver powder crystalline silicon based solar battery and preparation method thereof
CN103903675A (en) * 2012-12-28 2014-07-02 北京中科纳通科技有限公司 High-stability conductive slurry and preparation method thereof
JP2015156260A (en) * 2014-02-19 2015-08-27 Dowaエレクトロニクス株式会社 Silver paste burning film and electronic component
CN108053916A (en) * 2017-12-19 2018-05-18 深圳先进技术研究院 A kind of pressureless sintering conductive silver paste and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN102290117A (en) * 2011-04-25 2011-12-21 深圳市唯特偶新材料股份有限公司 Low temperature-sintered nano silver paste and preparation method thereof
CN102646459A (en) * 2012-05-23 2012-08-22 湖南利德电子浆料有限公司 Silver paste for front face of mixed silver powder crystalline silicon based solar battery and preparation method thereof
CN103903675A (en) * 2012-12-28 2014-07-02 北京中科纳通科技有限公司 High-stability conductive slurry and preparation method thereof
JP2015156260A (en) * 2014-02-19 2015-08-27 Dowaエレクトロニクス株式会社 Silver paste burning film and electronic component
CN108053916A (en) * 2017-12-19 2018-05-18 深圳先进技术研究院 A kind of pressureless sintering conductive silver paste and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111354514A (en) * 2020-03-06 2020-06-30 深圳第三代半导体研究院 Packaging paste based on multi-dimensional nano material and preparation method thereof
CN111354514B (en) * 2020-03-06 2021-06-22 深圳第三代半导体研究院 Packaging paste based on multi-dimensional nano material and preparation method thereof
CN113284645A (en) * 2021-04-25 2021-08-20 广州汉源新材料股份有限公司 Nano silver paste and preparation method thereof
CN114334221A (en) * 2022-01-10 2022-04-12 珠海方正科技多层电路板有限公司 Hole plugging copper paste, preparation method thereof and printed circuit board
CN114334221B (en) * 2022-01-10 2024-02-09 珠海方正科技多层电路板有限公司 Plug hole copper paste, preparation method thereof and printed circuit board
CN115810439A (en) * 2022-12-02 2023-03-17 广东华智芯电子科技有限公司 Silver-containing composite slurry, preparation method thereof and electronic interconnection material
CN116313223A (en) * 2023-03-28 2023-06-23 深圳市众诚达应用材料科技有限公司 Silver colloid and preparation method thereof
CN116313223B (en) * 2023-03-28 2024-05-28 深圳众诚达应用材料股份有限公司 Silver colloid and preparation method thereof

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Application publication date: 20190705